In 2266, CommanderSpock suggested that a truth serum be used on uncooperative Robert Crater, so as to determine the location of the salt vampire on the surface of M-113. The salt vampire in disguise as DoctorLeonard McCoy resisted the suggestion of using it, but was in favor of it, in this case, so as not to raise suspicion. Crater, unfortunately, was killed by the salt vampire prior to the administration of the drug. (TOS: "The Man Trap")

When Thelev was discovered to be an Orionspy serving in the Andorian delegation aboard the USS Enterprise, in 2268, he was subjected to questioning under a verifier scan and given truth drug. Unfortunately these tactics did not reveal anything, which suggested to Spock that his mind had been conditioned against such means as part of a preconceived plan. (TOS: "Journey to Babel")

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